Chinese Journal of Chromatography ›› 2019, Vol. 37 ›› Issue (2): 183-188.DOI: 10.3724/SP.J.1123.2018.10015

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Simultaneous determination of allopurinol, probenecid, benzbromarone in dietary supplements by ultra high performance liquid chromatography-tandem mass spectrometry

DENG Xingfei1,2, QI Yan1, LI Jinqing1, ZHANG Yan1, XIONG Bo1, LIU Hui1   

  1. 1. Guangdong Testing Institute of Product Quality Supervision, China National Quality Supervision and Testing Center for Food(Guangdong), Foshan 528300, China;
    2. South China Agricultural University, Guangzhou 510642, China
  • Received:2018-10-15 Online:2019-02-09 Published:2014-12-31
  • Supported by:

    Provincial Science and Technology Program in Guangdong Province (No. 2013B090600059).

Abstract:

A method based on QuEChERS purification was developed for the simultaneous determination of allopurinol, probenecid and benzbromarone in anti-gout dietary supplements by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted by acetonitrile mixed with 0.1% (v/v) ammonium hydroxide, and the extracts were purified using primary secondary amine (PSA) and C18 adsorbents. The samples were separated on a C18 chromatographic column with the gradient elution of 0.1% (v/v) formic acid aqueous solution and methanol as mobile phases. The analytes were detected by a electrospray ionization source in the positive or negative ion mode and the multiple reaction monitoring mode. The results showed that the limits of detection of allopurinol, probenecid and benzbromarone were 5, 25 and 25 μg/kg, and the limits of quantification were 17, 80 and 80 μg/kg. The average spiked recoveries of the three chemical drugs in dietary supplements were in the range of 76.8%-116.6% with the relative standard deviations of 2.7%-14.6%. The proposed method was applied for the analysis of 68 dietary supplements, and allopurinol was detected in one of them. This method is simple and sensitive, and can be used for the determination of the allopurinol, probenecid and benzbromarone in anti-gout dietary supplements.

Key words: allopurinol, benzbromarone, dietary supplements, probenecid, QuEChERS, ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

CLC Number: